GC Columns
Easy column selection for food testing Explore high performance GC phases Get featured food testing applications
Sensitive, Reproducible Results for Food Testingwith Zebron GC Columns
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Better Food Testing Starts Here
Zebron GC ColumnsServing Sensitive, Reproducible Performance Since 1998
p. 04 Easy Column Selection for Food Testing 04 The Master Resolution Equation 05 Selecting Your Dimensions 06 Selecting A Phase 08 Selection Charts for Food Testing
p. 10 Explore Premier Zebron Columns 10 Trust Guaranteed Quality By Design 11 ZB-1ms Low Bleed, High Sensitivity 12 ZB-SemiVolatiles The Ultimate Inert 5 Phase 13 ZB-5HT Inferno Rugged Performance to 430 14 ZB-MultiResidue-1 & -2 Separate Challenging Pesticides 15 ZB-WAXPLUS 100 % Aqueous Stability
p. 16 Featured Applications 16 Food Quality & Flavors Essential Oils Flavors Fatty Acids & FAMEs Sterols Triglycerides Spotlight: Alcoholic Beverages 24 Food Safety Additives & Preservatives Food Contact Materials Pesticides & Antimicrobials Environmental Contaminants Spotlight: Dioxins & PCBs
p. 34 Ordering Information
2015 Phenomenex, Inc. All rights reserved.
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Column LengthColumn ID
Carrier GasLinear Velocity
Column Phase
Temperature
Column IDFilm Thickness
Temperature
XX=Rs 4N
Retention Term
1
Selectivity TermEfficiency Term
1k
k
Relates to:
Otherconsiderations:
The Master Resolution Equation How do you choose a column? Do you reach into a cabinet of mystery columns, look to your favorite 5 % phenyl phase, or borrow one from a colleague? Understanding how column paramaters impact key elements of the master resolution equation will help you quickly make the right column selection for successful separations.
Phase Film Thickness
Polyimide CoatingFused Silica Glass
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GoodStarting Film
0.25 m
Thin Thick
Applications High boilers GC/MS applications Advantages Disadvantages Faster run times Less inert Higher temp. limits Limited retention Lower bleedHigherefficiency
0.10, 0.18 mApplications Low boilers Gases, solvents, purgeables, volatiles Purity testing Advantages Disadvantages Better inertness Slower run times Higher capacity Lower temp. limits Higher bleed
0.50 m or more
GoodStarting ID
0.25 mm
Narrow Wide
Applications Complex samples Advantages Faster run times Better resolution
0.10, 0.18, 0.20 mmApplications Dirty samples Highly concentrated samples Advantages Increased sample capacity Increased sample
0.32, 0.53 mm
Disadvantages Lower sample capacity Easily overloaded
Disadvantages Decreasedefficiency Mayneedhigherflow rates unsuitable for GC/MS
LengthLonger columns can improve resolution, but they will also increase run times. Under isothermal conditions, doubling column length only increases resolution by 41 %, but doubles the run time! Choose a column length that balances efficiency with accep-table run times.
Internal Diameter Column internal diameter (ID) has a major impact on both resolution and sample capacity. Unlike column length, using smaller ID columns can actually lead to faster run times, because the column length required with a small ID is often shorter due to increa-sed efficiency.
Film Thickness Film thickness determines solute retention and plays an important role in column sample capacity. Thin film columns are faster and provide higher resolution, but lower sample capacity. In most instances, choose the thinnest film possible that still provides adequate retention. When working with active samples, using a slightly thicker film can significantly improve peak shape.
GoodStarting Length
30 m
Short
ShortApplications High boilers GC/MS applications Advantages Disadvantages Faster run times Less inert Higher temp. limits Limited retention Lower bleedHigherefficiency
15 m or less Short 60 m or moreApplications Complex samples with closely eluting peaks Low boilers Less active samples Complex temperature ramps
Advantages Better resolution
Disadvantages Slow run times
Long
Selecting Your Dimensions
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Your Application
Requires
Phase
Your Sample Contains
100 % Dimethylpolysiloxane
Stable to 430 C for extended lifetime and high temp
bakeouts
ZB-1HT
100 % Dimethylpolysiloxane
Extremely versatile good starting point for boiling point
elutions
ZB-1
General purpose performance
100 % Dimethylpolysiloxane
Extremely versatile with reduced bleed for mass spectrometer analysis
ZB-1ms
Improved signal-to-noise ratios for better GC/MS
sensitivity
Non-polar analytes to be separated by true boiling point elution
High tempetaturecolumn diameters
< 0.53 mm
Selectivity Has The Biggest Impact On ResolutionResolution between two analytes is mainly determined by the selectivity of the stationary phase. By increasing resolution between two compounds, the total analysis time can often be reduced significantly. Phase polarity gives a general guideline for sample capacity and separation, which can affect peak shape and resolution. However, two columns may have similar polarity but show different separation profiles due to dissimilar selectivities. For example, ZB-35 and ZB-1701 are close in polarity, but the cyanopropyl group makes ZB-1701 different in terms of selectivity.
Selecting A Phase
Si OSi O
CH3
CH3
35 % Phenyl
65 % Dimethylpolysiloxane
ZB-35Polarity:18
Si O
CH3
CH3
86 % Dimethylpolysiloxane
Si O
(CH2 )3
NC
14 % Cyanopropylphenyl
ZB-1701Polarity:19
The 3 Most Prevalent GC InteractionsDispersive Forces (Van der Waals Interactions) Weakest of all intermolecular forces and occurs between non-polar compounds Separation is based on boiling point (classic example hydrocarbon separation in SimDist analysis)
Dipole-Dipole Interactions Either permanently present or induced by analyte-stationary phase interactions Higher dipole-dipole interaction can help separate compounds with similar boiling points, but different chemical structures
Hydrogen Bonding (Acid-Base Interactions) Can cause poor peak shape or irreversible binding to the inlet liner or to the column itself Zebron columns are specially deactivated to minimize these interactions
Choosing A 1 Phase (e.g. ZB-1)
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Your Application
Requires
Phase
Your Sample Contains
A wide range offunctional groups
Acids, Amines, BasesClosely eluting aromaticanalytes
High tempstability
0.53 mm IDor film > 0.50 m
Versatilityfor multiple
analyses
Good results foractive compounds
(food / environmental matrices)
Good results foractive compounds(pharmaceutical/
toxicology matrices)
5 % Phenyl
ZB-5HT
Stable to430 C
for extendedlifetime andhigh tempbakeouts
5 % Phenyl
ZB-5
Extremelyversatile
good startingpoint for a
typical 5 phase
5 % Phenyl-Arylene
ZB-5ms
Extremely versatilewith better
selectivity foraromatics
5 % Phenyl-Arylene
ZB-SemiVolatiles
Highly inert withequivalent selectivity toZB-5ms; recommended
for SVOCs, PBDEs,and active analytes
5 % Phenyl
ZB-5MSi
Highly inert withequivalent selectivity toZB-5; recommended for
drug screens andactive analytes
Your Application
Requires
Phase
Your Sample Contains
Polyethylene Glycol
ZB-WAXPLUS
Nitroterephthalic AcidModified Polyethylene Glycol
Excellent peak shape for
underivatized acids,organic acids, free fatty acids,
and alcohols
ZB-FFAP
Polyethylene Glycol
ZB-WAX
FAMEs, Flavors, Essential Oils, Solvents, or BTEXCompounds
Free Fatty Acids orOrganic Acids
100 % aqueous stabilitywith excellent separationsof polar complex mixtures;
widely used forprofiling and "fingerprinting"
General-purposePEG phase for polar
food samples
Aqueous stability for polar compounds;
low temperature volatiles
Improved signal-to- noise ratio for better
GC/MS sensitivity
Efficiency and inertness for acidic
analytes
Selecting A PhaseChoosing A 5 Phase (e.g. ZB-5)
Choosing A PEG Phase (e.g. ZB-WAX)
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Compound Class Analysis Recommended ColumnsPesticides & Antimicrobials Multi-Residue Pesticide Screening ZB-MultiResidue
-1 and 2
Organochlorine Pesticides in Water ZB-MultiResidue-1 and 2
Organochlorine Pesticides in Foods of Plant Origin ZB-MultiResidue-1 and 2
Organophosphorus Pesticides in Foods of Plant Origin ZB-MultiResidue-1 and 2
Triazine Pesticides in Water ZB-50
Triazine Pesticides in Foods of Plant Origin ZB-50
Chloramphenicol in Foods of Animal Origin ZB-1ms
Environmental Contaminants Polybrominated Diphenyl Ethers (PBDEs) in Food ZB-SemiVolatiles or ZB-35Polychlorinated Biphenyls (PCBs) in Water ZB-MultiResidue-1 or ZB-XLB-HT Inferno
Polychlorinated Dibenzo-dioxins (PCDDs) in Food ZB-5ms
Polychlorinated Dibenzo-furans (PCDFs) in Food ZB-5ms
Polycyclic Aromatic Hydrocarbons (PAHs) in Water ZB-SemiVolatiles or ZB-35
Food Contact Materials Food Packaging Volatiles ZB-624Melamine in Food ZB-XLB-HT Inferno
Cyanuric Acid in Food ZB-XLB-HT Inferno
Phthalates in Food ZB-5ms
Residual Solvents in Food ZB-624 or ZB-WAXPLUS
Bisphenol A & F (BPA/BPF) in Food ZB-5ms
Additives & Preservatives Parabens in Food ZB-5msChloropropanols (3-MCPD) in Food ZB-5ms
Flavor Additives (Borneol) ZB-MultiResidue-1
Phenolic Antioxidants (BHA & BHT) in Food ZB-50
Tocopherols in Food ZB-5
Process Contaminants Acrylamide in Foods ZB-5HT InfernoAcrylamide, Acrylonitrile, and Acrolein in Water ZB-624
Benzene in Food ZB-WAXPLUS
Glycols in Food ZB-WAXPLUS
Hormones Steroid Hormones in Food ZB-5ms or ZB-1ms
Compound Class Analysis Recommended ColumnsEssential Oils Cold-Pressed Orange Oil ZB-WAXPLUS
Ginkgo Biloba Oil ZB-1ms
Lavender Oil ZB-1ms
Peppermint Oil ZB-WAX
Rose Oil ZB-XLB
Spearmint Oil ZB-5ms
Ylang Ylang Oil ZB-1ms
Flavors Flavors Screening ZB-FFAPFlavor Allergens ZB-5ms
Flavor Volatiles ZB-1ms, ZB-WAXPLUS, or ZB-624
Alcoholic Beverage Profile ZB-FFAP
Honey Profile ZB-WAXPLUS
Fragrances Fragrance Screening ZB-WAXPLUS or ZB-624Fragrance Allergens ZB-1ms
Food Safety
Compound Class Analysis Recommended ColumnsFatty Acids & FAMEs Food Industry Fatty Acid Methyl Esters (FAMEs) ZB-WAXPLUS
Marine Oil Fatty Acid Methyl Esters (FAMEs) ZB-WAXPLUS
Saw Palmetto Fatty Acid Methyl Esters (FAMEs) ZB-WAXPLUS
Free Fatty Acids ZB-FFAP
Essential Fatty Acids (EFAs) Omega-3 and Omega-6 ZB-WAXPLUS
Triglycerides Butter Triglycerides ZB-5HT InfernoCanola Oil Triglycerides ZB-5HT Inferno
Olive Oil Triglycerides ZB-5HT Inferno
Peanut Oil Triglycerides ZB-5HT Inferno
Alcoholic Beverages Cognac Compounds ZB-WAXPLUSDistilled Liquor Screen ZB-FFAP
Ethanol in Beer ZB-Bioethanol
Sulfur in Beer ZB-1ms
Whiskey Compounds ZB-WAXPLUS
Wine Compounds ZB-WAX or ZB-WAXPLUS
Other Acids Organic Acids ZB-FFAPAmino Acids ZB-50
Sterols Sterols in Lard ZB-5HT InfernoSterols in Margarine ZB-5HT Inferno
Sterols in Olive Oil ZB-5HT Inferno
Sterols in Peanut Butter ZB-5HT Inferno
Sugars Alditol Acetates ZB-5msTrimethylsilyl (TMS) Sugars ZB-MultiResidue-1
Food Quality
Flavors & Fragrances
GC Column Selection by Application
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Zebron Phase Zebron Composition Restek Agilent Supelco Alltech SGE OV
ZB-1 100 % DimethylpolysiloxaneRtx-1, Rtx-1PONA, Rtx-1 F&F
DB-1, DB-2887, DB-1 EVDX,HP-1, HP-101, HP-PONA,Ultra 1, CP-Sil 5 CB
SPB-1, SPB-1 TG, SE-30, MET-1, SPB-1 Sulfur, SPB-HAP
AT-1, AT-Sulfur, EC-1
BP1, BP1-PONA, BPX1-SimD
OV-1
Featuredon p. 11 ZB-1ms 100 % Dimethylpolysiloxane Rtx-1ms
DB-1ms, HP-1ms, CP-Sil 5 CB MS, VF-1ms
MDN-1, Equity-1 AT-1ms SolGel-1ms
ZB-1HT Inferno 100 % Dimethylpolysiloxane Rxi-1HT DB-1ht, CP-SimDist Petrocol 2887
ZB-1XT SimDist 100 % Dimethylpolysiloxane MXT-1HT SimDist CP-SimDist UltiMetal DB-HT SimDis
ZB-5 5 % Phenyl 95 % Dimethylpolysiloxane Rtx-5DB-5, HP-5, Ultra 2, HP-PAS-5, CP-Sil 8 CB
MDN-5, SPB-5, PTE-5, SE-54, PTA-5, Equity-5, Sac-5
AT-5, EC-5 BP5, BPX5 OV-5
ZB-5MSi 5 % Phenyl 95 % DimethylpolysiloxaneRtx-5ms, Rxi-5ms, Rtx-5Amine
DB-5, HP-5ms, HP-5msi, HP-5ms Ultra Inert MDN-5S
Featuredon p. 13 ZB-5HT Inferno
5 % Phenyl 95 % Dimethylpolysiloxane
Stx-5HT, Rxi-5HT, XTI-5HT, Rtx-5HT DB-5ht, VF-5ht HT-5
ZB-5ms 5 % Phenyl-Arylene 95 % DimethylpolysiloxaneRtx-5Sil MS,Rxi-5Sil MS
DB-5ms, DB-5.625, DB-5ms EVDX, VF-5ms, CP-Sil 8 CB MS
Featuredon p. 12 ZB-SemiVolatiles
5 % Phenyl-Arylene 95 % Dimethylpolysiloxane
Rxi-5Sil MSRxi-5ms
DB-5ms Ultra InertHP-5ms Ultra Inert SLB
-5ms
ZB-35 35 % Phenyl 65 % DimethylpolysiloxaneRtx-35, Rtx-35ms
DB-35, DB-35ms, HP-35, HP-35ms
MDN-35, SPB-35, SPB-608 AT-35 BPX35, BPX608 OV-11
ZB-35HT Inferno35 % Phenyl 65 % Dimethylpolysiloxane Phenomenex Exclusive
ZB-50 50 % Phenyl50 % Dimethylpolysiloxane Rtx-50DB-17, DB-17HT, DB-17ms, DB-17 EVDX, HP-50+, CP-Sil 24 CB
SP-2250, SPB-17, SPB-50 AT-50 BPX50 OV-17
ZB-624 6 % Cyanopropyl phenyl 94 % DimethylpolysiloxaneRtx-1301, Rtx-624
DB-1301, DB-624, DB-VRX, HP-VOC, CP-1301, CP-Select 624 CB
SPB-1301, SPB-624 AT-624, AT-1301 BP624 OV-624
ZB-1701 14 % Cyanopropyl phenyl 86 % Dimethylpolysiloxane Rtx-1701 DB-1701 , CP-Sil 19 CB SPB-1701, Equity-1701 AT-1701 BP10 OV-1701
ZB-1701P 14 % Cyanopropyl phenyl 86 % Dimethyl polysiloxane DB-1701P
ZB-WAX Polyethylene glycol Rtx-WAX, Famewax,Stabilwax-DB
DB-WAXetr, HP-INNOWax, CP-Wax 57 CB Met-Wax, Omegawax EC-Wax SolGel-WAX
Featuredon p. 15 ZB-WAXPLUS
Polyethylene glycol StabilwaxDB-WAX, CAM, HP-20M, Carbowax 20M, CP-Wax 52 CB
SUPELCOWAX 10 AT-Wax, AT-AquaWax BP20Car-bowax 20M
ZB-FFAP Nitroterephthalic acid modified polyethylene glycol Stabilwax-DADB-FFAP, HP-FFAP, CP-Wax 58 (FFAP) CB, CP-FFAP CB
Nukol, SPB-1000 AT-1000, EC-1000 BP21 OV-351
ZB-CLPesticides-1 Proprietary Rtx-CLPesticides, Stx-CLPesticides
ZB-CLPesticides-2 Proprietary Rtx-CLPesticides2, Stx-CLPesticides2
Featuredon p. 14 ZB-MultiResidue
-1 Proprietary Rtx-CLPesticides, Stx-CLPesticides
ZB-MultiResidue-2 Proprietary Rtx-CLPesticides2, Stx-CLPesticides2
ZB-XLB Proprietary Rtx-XLB DB-XLB, VF-XMS MDN-12
ZB-XLB-HT Inferno Proprietary Phenomenex Exclusive
ZB-Drug-1 Proprietary Phenomenex Exclusive
ZB-BAC-1 Proprietary Rtx-BAC1 DB-ALC1
ZB-BAC-2 Proprietary Rtx-BAC2 DB-ALC2
ZB-Bioethanol Proprietary Phenomenex Exclusive
This section is, neither in terms of manufacturers nor in terms of their products, a complete list, and the accuracy of the data is not guaranteed. Small differences in dimensions or performance might be possible and slight adjustments to your application may be necessary.*See p. 10
Upgrade to Zebron! Our commitment to quality and innovation is what makes Zebron GC columns well suited for any application. Performance is GUARANTEED*.
GC Column Selection by Manufacturer
Looking For Another Phase?Well cross-reference your current column for you! Contact your local GC Specialist for additional information or visit www.phenomenex.com/GC
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Guaranteed Quality by DesignOur GC R&D and production team has on average 25+ years of GC experience, and many spent years creating keystone phases at J&W Scientific prior to joining the Phenomenex team. This expertise means Zebron products are designed to work out-of-the-box, headache free. We guarantee it.
Stringent individual QC testing no batch tests
Excellent sensitivity and high temperature stability
MS certified phases for low bleed
Novel selectivities for better separations
Explore PremiereZebron GC Columns
Explore ZebronTM Phases for Food Testing
Were YouTube Stars!
www.phenomenex.com/InnovateGC
Were so committed to quality, we made a video about it! Watch it at
Better Quality, Less Maintenance After most runs with Zebron, I didnt have to clean or trim the column. The separation was the same, but the Zebron lasted about 4-5 times longer, which for me means saving at least $5,000 a year.
Sam SabellaBASF USA
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If Zebron columns do not provide you with equivalent or better separations as compared to any other GC column of the same phase and comparable dimensions, send in your comparative data within 45 days and keep the col-umn for FREE!
5
POLARITY
USP PHASEG1, G2, G9, G38
MS CERTIFIED
TEMP LIMITS C-60 to 360/370
The Ultimate MS Certified 1 Phase Column Profile
Phase Chemistry
Recommended Applications Acids
Amines
Essential Oils
Flavors
Fragrances & Fragrance Allergens
Oxygenates
PCBs
Pesticides
Solvent Impurities
Sulfur Compounds (Light)
Very low bleed phase especially suited to high sensitivity GC/MS Extremely inert for active compounds such as pesticides, or acids
and bases Improved signal-to-noise ratio for better sensitivity and mass
spectral integrity Identical selectivity to ZB-1
Lower Overall Column ActivityActivity is a key measure of column quality. Zebron ZB-1ms columns are aggressively tested to ensure full deactivation. Below is an example of the stringent QC test mix we use, notice the low tailing for even the most active compounds like 2-Ethylhexanoic Acid!
Test Conditions for Zebron ZB-1ms
Column: Zebron ZB-1ms Dimensions: 30 meter x 0.25 mm x 0.25 m
Part No.: 7HG-G011-11Injection: Split @ 250 C, 1.0 L
Carrier Gas: Hydrogen @ 1.18 mL/min (constant flow)Oven Program: 140 C (Isothermal)
Detector: FID @ 325 CSample: 1. Decane
2. 2-Ethylhexanoic Acid 3. 4-Chlorophenol 4. Naphthalene 5. Tridecane 6. 1-Undecanol 7. Dicyclohexylamine 8. Pentadecane
1 2 3 4
1
2
35
4
6 7
8
5 6 7 8 9 10 min
App
ID 1
5545
Upgrade to ZebronTM from any 100 % dimethylpolysiloxane phase:Agilent Alltech Restek SGE SupelcoDB-1 AT-1 Rtx-1 BP1 SPB-1
DB-1ms AT-1ms Rtx-1ms SolGel-1msTM SE-30
DB-1ms Ultra Inert EC-1 Rxi-1ms MET-1
HP-1 MDN-1
HP-1ms Equity-1
HP-1ms Ultra Inert
VF-1ms
CP-Sil 5 CB
Ultra 1
ZB-1ms
Si O
CH3
CH3100 % Dimethylpolysiloxane
Explore PremiereZebron GC Columns
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POLARITY
USP PHASEG27, G36, G41
MS CERTIFIED
TEMP LIMITS C-60 to 325/350
Comparative separations may not be representative of all applications.
Specificallydesignedtoovercomeobstaclesforsensitivemethods
Enviro-InertTM Technology provides improve inertness without compromising selectivity
Our column of choice for acids, bases, amines, and other active compounds
Improve Inertness for Active Compounds Pyridine is a very active amine and a good indicator for both column lifetime and sensitivity. Columns with higher initial peak responses can be expected to maintain performance over time. Higher responses also allow you to run at lower levels of detection, improving sensitivity.
Upgrade to ZebronTM from any 5 % phenyl or 5 % phenyl-arylene / 95 % dimethylpolysiloxane phase:Agilent Restek SupelcoDB-5ms HP-5ms Rxi-5Sil MS SLB-5ms
DB-5ms Ultra Inert HP-5ms Ultra Inert Rxi-5ms
DB-5.625 VF-5ms Rxi-1ms
CP-Sil 8 CB MS
Inte
nsity
(pA
)
9.00
11.00
13.00
15.00
17.00
19.00
2.50 2.70 2.90 3.10 3.30 3.50 3.70 3.90 min
ZB-SemiVolatiles
DB-5ms Ultra Inert
Rxi-5Sil MS
Rxi-5ms
HP-5ms Ultra Inert
min
Customer Approved!
I have found the Phenomenex ZB-SemiVolatiles columns to be superior in quality and durability than any other columns we have previously used. The columns not only last longer, but the reproducibility of column is extraordinary. The column holds calibrations particularly well, even after multiple injections of samples with far less than desirable matrices. All of this equates to less downtime and maintenance and more productivity for TestAmerica. Ryan McKernan, GC/MS Semi-Volatile Analyst
TestAmerica Laboratories, Inc. Buffalo
Recommended Applications Semivolatiles (SVOCs)
Polycyclic Aromatic Hydrocarbons (PAHs)
Polybrominated Diphenyl Ethers (PBDEs)
Active Compounds, Acids, Bases
Phase Chemistry
Si O
CH3
CH395 % Dimethylpolysiloxane5 % Phenyl
Si O
Get Best-In-Class Performance Column Profile
ZB-SemiVolatiles
8
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POLARITY
USP PHASEG27, G36, G41
MS CERTIFIED
TEMP LIMITS C-60 to 400/430*
Comparative separations may not be representative of all applications.
First non-metal columns stable to 430 C Robust column well suited for analysts struggling with high
boilers, contaminants, or carryovers Longer lifetime with rugged high temperature, polyimide
coated, fused silica tubing Low activity, provides good peak shape for acidic and basic
samples Individuallytestedforlowbleed,MScertified
Upgrade to ZebronTM from any 5 % phenyl / 95 % dimethylpolysiloxane phase:Agilent Alltech Restek SGE SupelcoDB-5ht AT-5 Stx-5HT BP5 HT-5
DB-5 EC-5 XTI-5HT BPX5
HP-5 Rtx-5
VF-5ht Rxi-5HT
Recommended Applications Semivolatiles (SVOCs)
Polycyclic Aromatic Hydrocarbons (PAHs)
Polybrominated Diphenyl Ethers (PBDEs)
Active Compounds, Acids, Bases
Phase Chemistry
Recommended Applications Dirty or Highly Contaminated Samples
High Boiling Compounds
High Molecular Weight Waxes
Hydrocarbon Separations
Polymers/Plastics
Sterols
Triglycerides
Conditions for all columns:Dimensions: 30 meter x 0.25 mm x 0.10 m
Injection: 1.0 L of test mix AG0-7578 Carrier Gas: Helium @ 1.9 mL/min (constant flow)
Oven Program: 120 C (Isothermal)Detector: Flame Ionization Detector (FID) @ 400 C
Sample: Pentadecane
How does the lifetime test work?For the test, all columns were held at 400 C for 2 hours and then the oven was lowered to 120 C for Pentadecane analysis. Pentadecane retention between Zebron ZB-5HT Inferno and other traditional 5 % Phenyl 95 % dimethylpolysiloxane column was compared. The VF-5ht column died around 40 hours at 400 C whereas ZB-5HT Inferno maintained great retention of pentadecane over 100 hours over 2X the lifetime!
6
6.5
7
7.5
8
8.5
0 20 40 60 80 100 120
Ret
entio
n of
Pen
tad
ecan
e at
120
C
(min
)
Hours at 400 C
Zebron ZB-5HT Inferno Agilent DB-5ht Agilent VF-5ht Si O
CH3
CH395 % Dimethylpolysiloxane5 % Phenyl
Si O
Robust Performance Up To 430 C Column Profile
ZB-5HT InfernoTM
8
* 0.53 mm ID columns are rated to 400 C.
2x the lifetime!
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Proprietary phases specially designed for the separation of all types of pesticides, herbicides, and insecticides
Reliable performance for multi-residue screens by GC/MS Low activity, decreased breakdown of sensitive pesticides
such as DDT Provides robust column performance for high temperature
bake outs
Upgrade to ZebronTM from these similar* phases:Agilent Restek
DB-CLP1 Rtx-CLPesticides
DB-CLP2 Rtx-CLPesticides2
Stx-CLPesticides
Stx-CLPesticides2
Recommended Applications Haloacetic Acids (HAAs)
Herbicides / Insecticides
Multi-Pesticide Screening
Nitrogen Containing Pesticides
Organochlorine Pesticides
Organophosphorous Pesticides
PCBs / Aroclors
Phase Chemistry
ZB-MultiResidue-1 & -2Optimized Results for Pesticides
Perform Challenging Separations
*not exact equivalent, selectivity might be different
POLARITY MS CERTIFIED
TEMP LIMITS C-60 to 320/340
15
MR-1
10 10.5 11
1
23
4 5
6
11.5 12 12.5 min
Sample:
1. o,p-DDE
2. p,p-DDE
3. o,p-DDD
Cl
Cl Cl
ClCl
Cl Cl
ClCl
Cl
ClCl
Cl
ClCl
ClCl
Cl
Cl
ClCl
Cl
Cl ClCl
Cl
4. o,p-DDT
5. p,p-DDD
6. p,p-DDTCl
Cl Cl
ClCl
Cl Cl
ClCl
Cl
ClCl
Cl
ClCl
ClCl
Cl
Cl
ClCl
Cl
Cl ClCl
Cl
Acquisition Spectra
NIST Reference Spectra
20 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380
0200400600800
10001200140016001800200022002400
Abundancia m/z-->
235165
199
75 88 105113
28250
251
20 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 4000
200400600800
10001200140016001800200022002400
Abundancia m/z-->
235165
199
88123105
50281 35431914928 69
App
ID: 1
6161
DDT, DDD, and DDE Isomer Separation at 25 ng On-Column
Proprietary
11
POLARITY MS CERTIFIED
TEMP LIMITS C-60 to 320/340
Column Profile
MR-1
MR-2
Low Bleed No 207 bleedions at 320
Abundance
Abundance
Phenomenex l Web: www.phenomenex.com Phenomenex l Web: www.phenomenex.com14 15
POLARITY
USP PHASEG14, G15, G16G20, G39, G47
TEMP LIMITS C20 to 250/260*
Comparative separations may not be representative of all applications.
Excellent for water samples Extremely inert for acidic compounds Enhanced selectivity for low boiling solvents High retention of alcohols and chlorinated solvents
Upgrade to ZebronTM from any polyethylene glycol phase:Agilent Alltech Restek SGE SupelcoDB-WAX AT-Wax Stabilwax BP20 SUPELCOWAX 10
CAM AT-AquaWax
HP-20M
Carbowax 20M
CP-Wax 52 CB
Recommended Applications Haloacetic Acids (HAAs)
Herbicides / Insecticides
Multi-Pesticide Screening
Nitrogen Containing Pesticides
Organochlorine Pesticides
Organophosphorous Pesticides
PCBs / Aroclors
Phase Chemistry
Recommended Applications Alcohols & Alcoholic Beverages
Aldehydes
Aromatics
Essential Oils
Fatty Acid Methyl Esters (FAMEs)
Flavors & Fragrances
Glycols
OVIs
Solvents / Residual Solvents
ZB-WAXPLUS100 % Aqueous Stability for Polar Compounds
Column Profile
2
1
2
3
4
5
6
7
8
9
10
11
12
13 1415
16
17
3 4 5 6 7 min
Zebron ZB-WAXplus
App
ID 1
5815
2
1
2
3
5
46
7
8,9
10
11
12
13 1415
16
17
3 4 5 6 7 min
App
ID 1
5816
Restek Stabilwax
Conditions same for both columns:Dimensions: 30 meter x 0.25 mm x 0.25 m
Injection: Split 100:1 @ 250 C, 1 L Carrier Gas: Hydrogen @ 1.0 mL/min (constant flow)
Oven Program: 5 C for 2.5 min to 85 C at 10 C/min and hold until last peak elutes
Detector: FID @ 225 CSample: 1. Methyl Formate
2. Acetone 3. Ethyl Acetate 4. Methyl Ethyl Ketone 5. Methanol 6. 2-Methyl-2-propanol 7. Methylene Chloride 8. Benzene 9. Ethanol
10. 2-Butanol 11. Toluene 12. n-Propanol 13. Ethyl Benzene 14. p-Xylene 15. m-Xylene 16. 1-Butanol 17. o-Xylene
* Thicker films ( 1.0 m) are rated to 230/240 C.
100 % Polyethylene Glycol (PEG)
O O
H
H
H
H
C C
52
ImproveResolution
Phenomenex l Web: www.phenomenex.com Phenomenex l Web: www.phenomenex.com14 15
Cold-Pressed Orange Oil by GC/MS ZB-WAXplus 60 m x 0.25 mm x 0.25 m ZB-WAXplus 10 m x 0.10 mm x 0.10 m
Column: ZB-WAXPLUSDimensions: 60 meter x 0.25 mm x 0.25 m
Part No.: 7KG-G013-11Injection: Split 40:1 @ 220 C, 0.1 L
Carrier Gas: Helium @ 1.2 mL/min (constant flow)Oven Program: 40 C for 0.2 min to 210 C @
10 C/min for 10 minDetector: MSD; 45-450 amu
Column: ZB-WAXPLUSDimensions: 10 meter x 0.10 mm x 0.10 m
Part No.: 7CB-G013-02Injection: Split 20:1 @ 220 C, 0.2 L
Carrier Gas: Helium @ 0.3 mL/min (constant flow)Oven Program: 35 C for 1 min to 250 C @ 30 C/min for 5 min
Detector: MSD; 45-450 amu
1. a-Pinene 2. b-Pinene 3. Sabinene 4. 3-Carene 5. b-Myrcene 6. Limonene 7. b-Phellandrene 8. Octanal 9. Nonanal 10. Limonene Oxides 11. Citronellal 12. Decanal 13. a-Cubebene 14. Linalool 15. b-Cubebene 16. Octanol
17. Germacrene 18. Caryophyllene 19. trans-p-Mentha-2,8- 20. cis-p-Mentha-2,8- 21. Gerenial 22. a-Terpineol 23. Dodecanal 24. Valencene 25. Citral 26. Carvone 27. Cadinene 28. Perillaldehyde 29. trans-Carveol 30. cis-Carveol 31. Perillol 32. Octanoic acid
Sample:
dienoldienol
7 8 9 10 11 12 13 14 15 16 17 18 19 20 min
1
2
3
4
5 6
7
8
9
10
11
12 14
13
16
1517
18
1920
21
22 25
24
23
26
27
28
29
30
3132
65% FAsTER!
App
ID 1
5811
2 2.50 3 3.50 4 4.50 5 5.50 6 min
1
2
3
4
56
7
8
9
10
11
12 14
13 1516
17
18
19 2021
22
23
26
24,25
27
28
29
3031
32
Maintain separation with faster run times
Essential OilsEssential oils are fragrant plant essences primarily composed of terpenes, their derivatives, and other aromatic compounds. Variation in plant location and growing conditions produces natural differences in essential oil components, and due to their high price, premium oils are subject to adulteration with cheaper terpenes or poorer quality oils. Characterization of essential oils is therefore necessary, but testing is complex due to the number of compounds and their trace level presence. Runs under seven minutes can be achieved using efficient column dimensions, as demonstrated below.
Flavors
App
ID 1
5812
Explore PremiereZebron GC Columns
Food Quality & FlavorsFeatured Applications
Phenomenex l Web: www.phenomenex.com Phenomenex l Web: www.phenomenex.com16 17
Essential OilsFlavorsRosemary Oil by GC/MS
Column: ZebronTM ZB-1msDimensions: 10 meter x 0.10 mm x 0.10 m
Part No.: 7CB-G011-02Injection: Split 120:1 @ 160 C, 0.2 L
Carrier Gas: Helium @ 0.4 mL/min (constant flow) Oven Program: 45 C for 2 min to 130 C @ 8 C/min to
200 C @ 30 C/min for 2 minDetector: MSD; 18-400 amu
Sample: Sample was 10 % in dichloromethane 1. Tricyclene 2. a-Thujene 3. a-Pinene 4. Camphene 5. b-Pinene 6. b-Myrcene 7. Eucalyptol
8. Limonene 9. g-Terpinene 10. Terpinolene 11. Linalool 12. Camphor 13. Isoborneol 14. Borneol
15. 4-Terpineol 16. Terpineol 17. Bornyl Acetate 18. Eugenol 19. Copaene 20. Caryophyllene 21. a-Caryophyllene
Peppermint Oil by GC/MS Column: Zebron ZB-1ms
Dimensions: 10 meter x 0.10 mm x 0.10 mPart No.: 7CB-G011-02Injection: Split 120:1 @ 160 C, 0.2 L
Carrier Gas: Helium @ 0.3 mL/min (constant flow)Oven Program: 45 C for 2 min to 130 C @ 10 C/min to
280 C @ 30 C/min for 3 minDetector: MSD
Sample: Analytes are 10 % in dichloromethane 1. a-Pinene 2. Sabinene 3. b-Pinene 4. b-Myrcene 5. 3-Octanol 6. a-Terpenene 7. Cymene 8. Eucalyptol 9. d-Limonene10. cis-Ocimene11. trans-Ocimene
12. g-Terpinene13. cis-Sabinene hydrate14. b-Terpineol15. Linalool16. Menthone17. Isomenthone18. Menthonefuran19. Neomenthol20. Menthol21. Neoisomenthol22. a-Terpineol
23. Pulegone24. Piperitone25. Neomenthyl acetate26. Menthyl acetate27. Isomenthyl acetate28. Bourbonene29. Caryophyllene30. Farnesene31. Germacrene32. Elemene
3 4
12
4 53
5 6
6
7 8
7,8
9
9
10
10
11
11
12
12
13
13
15
16 17
18 19
20
21
14
14
min
3 4 5 6 7 8 9 10 11 12 min
1
2
3
4,5
67
8
9
1011
12
13
14 15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
16018
App
ID 1
6070
App
ID 1
6018
Ylang Ylang Oil by GC/MS Column: Zebron ZB-1ms
Dimensions: 10 meter x 0.10 mm x 0.10 mPart No.: 7CB-G011-02Injection: Split 120:1 @ 160 C, 0.2 L
Carrier Gas: Helium @ 0.5 mL/min (constant flow)Oven Program: 60 C to 120 C @ 15 C/min to 160 C @ 5 C/min to
220 C @ 20 C/minDetector: MSD; 18-400 amu
Sample: Oil was 10 % in dichloromethane 1. p-Methyl anisole 2. Methyl benzoate 3. Linalool 4. Benzyl acetate 5. Geraniol 6. Geranyl acetate
7. Copaene 8. b-Caryophyllene 9. Cinnamyl acetate 10. Humulene 11. Germacrene 12. a-Amorphene
13. Farnasene 14. d-Cadinene 15. Farnesol 16. Benzyl benzoate 17. Benzyl salicylate 18. Farnesyl acetate
Spearmint Oil by GC/MS Column: Zebron ZB-1ms
Dimensions: 10 meter x 0.10 mm x 0.10 mPart No.: 7CB-G011-02Injection: Split 120:1 @ 160 C, 0.2 L
Carrier Gas: Helium @ 0.4 mL/min (constant flow)Oven Program: 45 C for 2 min to 130 C @ 8 C/min to
200 C @ 30 C/min for 2 minDetector: MSD; 18-400 amu
Sample: Analytes are 10 % in dichloromethane 1. 2,5-Diethyltetrahydrofuran 2. a-Pinene 3. abinene 4. b-Pinene 5. b-Myrcene 6. 3-Octanol 7. Eucalyptol 8. Limonene 9. cis-Sabinene hydrate10. Menthone11. Isomenthone12. 4-Terpineol
13. Dihydrocarveol14. Carvone15. Piperitenone16. trans-Carvone oxide17. cis-Carvone oxide18. Carvyl acetate19. cis-Jasmone20. b-Bourbonene21. Caryophyllene22. b-Farnesene23. Germacrene D24. Caryophyllene oxide
2
1
2
3
3
4
4
5
5
6
6
7
7
8
8,9
9 10
10
11
11
12
12
13
13
14
14
15
15
18
1718
min
2
3
2
4
1
4
6
5,6
8
8
7
10
10
9
12
12
11
13
14
14
16
17
18
19
20
21
22
23
2416
min
16048
15
App
ID 1
6053
App
ID 1
6048
Explore PremiereZebron GC Columns
Phenomenex l Web: www.phenomenex.com Phenomenex l Web: www.phenomenex.com16 17
Flavor ScreeningAromas can be exceedingly complex, with several hundred compounds playing a role. Polyethylene glycol (PEG) phases are routinely used for flavor analysis; common phases (ZB-WAX and ZB-FFAP) used for flavor screening are demonstrated below.
Flavors
Flavors Analysis by GC/MS
Flavors Analysis by GC/MS Column: Zebron ZB-FFAP
Dimensions: 30 meter x 0.25 mm x 0.25 mPart No.: 7HG-G009-11Injection: Split 100:1 @ 250 C, 1 L
Carrier Gas: Helium @ 1 mL/min (constant flow)Oven Program: 50 C to 250 C @ 6 C/min for 3 min
Detector: MSD @ 270 CSample: 1. Acetone
2. Ethyl Acetate 3. Ethanol 4. Decane 5. Ethyl Butyrate 6. Limonene 7. 2,3-Dimethylpyrazine 8. (z)-3-Hexenol 9. Tetradecane
10. Acetic Acid 11. Decanal 12. Propylene Glycol 13. Ethyl Decanoate 14. Neral 15. a-Terpineol 16. Neryl Acetate 17. Geranial 18. Valeric Acid
19. Decanol 20. Nonanoic Acid 21. Decanoic Acid 22. Vanillin 23. Anthracene
0
2
1
3
4
5
6
7 8
9
10
1112
13
14
1516
17
18
20
21
22
23
19
5 10 15 20 25 30 min
0
1
2
3
4
5
6
78
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
5 10 15 20 25 30
14900
min
App
ID 1
4899
Test mix courtesy of Frutarom (UK) Ltd., Flavour Chemistry Laboratory.
Column: Zebron ZB-WAXDimensions: 30 meter x 0.32 mm x 0.25 m
Part No.: 7HG-G007-11Injection: Split 100:1 @ 250 C, 1.0 L
Carrier Gas: Helium @ 1 mL/min (constant flow)Oven Program: 50 C to 250 C @ 6 C/min for 3 min
Detector: MSD @ 275 CSample: 1. Acetone
2. Ethyl acetate 3. Ethanol 4. Decane 5. Ethyl butyrate 6. Limonene 7. 2,3-Dimethylpyrazine 8. (Z)-3-Hexenol 9. Tetradecane10. Acetic acid11. Decanal12. Propylene glycol13. Ethyl decanoate14. Neral15. a-Terpineol16. Neryl Acetate17. Geranial18. Decanol19. Valeric acid20. Nonanoic acid21. Decanoic acid22. Vanillin23. Anthracene
App
ID 1
4900
Phenomenex l Web: www.phenomenex.com Phenomenex l Web: www.phenomenex.com18 19
Fatty Acids & FAMEsFat and oil testing is important for both characterization as well as determination of total fat content. Both fatty acid methyl esters (FAMEs) and free fatty acids (FFAs) are commonly analyzed using polyethylene glycol (PEG) phases. The examples below display good resolution for both derivatized and underivatized fatty acids.
Fats & Oils
Unsaturated Fatty Acids Methyl Esters (FAMEs) by GC/FID Column: Zebron ZB-FFAP
Dimensions: 60 meter x 0.25 mm x 0.25 mPart No.: 7KG-G009-11Injection: Split 40:1 @ 220 C, 0.2 L
Carrier Gas: Helium @ 2.4 mL/min (constant flow)Oven Program: 200 C to 260 C @ 2 C/min for 30 min
Detector: FID @ 250 CSample: 1. Methyl Myristate
2. Methyl Myristoleate 3. Methyl Palmitate 4. Methyl Palmitelaidate 5. Methyl Palmitoleate 6. Methyl Stearate 7. Methyl Oleate 8. Methyl Elaidate 9. Methyl Linoleate
10. Methyl Linelaidate 11. Methyl Linolenate 12. Methyl Arachidate 13. Methyl Gondonate 14. Methyl Behenate 15. Methyl Erucate
Unsaturated Free Fatty Acids by GC/FID Column: Zebron ZB-FFAP
Dimensions: 60 meter x 0.25 mm x 0.25 mPart No.: 7KG-G009-11Injection: Split 40:1 @ 220 C, 0.2 L
Carrier Gas: Helium @ 2.4 mL/min (constant flow)Oven Program: 200 C to 260 C @ 2 C/min for 30 min
Detector: FID @ 250 CSample: 1. Myristic Acid
2. Myristoleic Acid 3. Palmitic Acid 4. Palmitelaidic Acid 5. Palmitoleic Acid 6. Stearic Acid 7. Elaidic Acid 8. Oleic Acid 9. Linolelaidic Acid
10. Linoleic Acid 11. Linolenic Acid 12. Arachidic Acid 13. Gondonic Acid (C15) 14. Behenic Acid (C17) 15. Erucic Acid (C19)
45 min30 35 402515 2010
1
23
45
6
7,8
9,10
11
12 1314
15
10
1
2
3
5
4
8
6
7
9
10
11
1213
14 15
15 20 25 30 35 40 min
App
ID 1
4856
App
ID 1
4858
Food Industry FAMEs by GC/FID Column: Zebron ZB-WAX
Dimensions: 30 meter x 0.25 mm x 0.25 mPart No.: 7HG-G007-11Injection: Split 5:1 @ 220 C, 1 L
Carrier Gas: Helium @ 3 mL/min (constant flow)Oven Program: 60 C for 2 min to 150 C @ 13 C/min to 240 C
@ 2 C/minDetector: FID @ 250 C
Sample: 133-266 ppm in methylene chloride
163201 2 3 4
5
6
7
8
9
10 11
12
1314
15
1617,18
1920 21 22
23
2425 26
27282930
31
32 33 34
35
36
37
201 10 30 40 min
1. Methyl Butyrate (C4:0)2. Methyl Hexanoate (C6:0)3. Methyl Octanoate (C8:0))4. Methyl Decanoate (C10:0)5. Methyl Undecanoate (C:11)6. Methyl Laurate (C12:0)7. Methyl Tridecanoate (C13:0)8. Methyl Myristate (C14:0)9. Myristoleic acid methyl ester (C14:1)
10. Methyl Pentadecanoate ( C15:0)11. cis-10-Pentadecenoic acid methyl ester (C15:1)12. Methyl Palmitate (C16:0)13. Palmitoleic acid methyl ester (C16:1)14. Methyl Heptadecanoate (C17:0)15. cis-10-Heptadecenoic acid methyl ester (C17:1)16. Methyl Stearate (C18:0)17. Oleic acid methyl ester (C18:1n9c)18. Elaidic acid methyl ester (C18:1n9t)19. Linoleic acid methyl ester (C18:2n6c)20. Linolelaidic acid methyl ester (C18:2n6t)21. g-Linolenic acid methyl ester (C18:3n6)22. Linolenic acid methyl ester (C18:3n3)23. Methyl Arachidate (C20:0)24. cis-11-Eicosenoic acid methyl ester (C20:1)25. cis-11-14-Eicosadienoic acid methyl ester (C20:2)26. cis-8,11,14-Eicosatrienoic acid methyl ester (C20:3n6)27. Methyl Heneicosanoate (C21:0)28. Arachidonic acid methyl ester (C20:4n6)29. cis-11,14,17-Eicosatrienoic acid methyl ester (C20:3n3)30. cis-5,8,11,14,17-Eicosapentaenoic acid methyl ester (C20:5n3)31. Methyl Behenate (C22:0)32. Erucic acid methyl ester (C22:1)33. cis-13,16-Docosadienoic acid methyl ester (C22:2)34. Methyl Tricosanoate (C23:0)35. Methyl Lignocerate (C24:0)36. cis-4,7,10,13,16,19-Docosahexaenoic acid methyl ester (C22:6n3)37. Nervonic acid methyl ester (C24:1)
App
ID 1
6320
Test mix courtesy of Frutarom (UK) Ltd., Flavour Chemistry Laboratory.
Column: Zebron ZB-WAXDimensions: 30 meter x 0.32 mm x 0.25 m
Part No.: 7HG-G007-11Injection: Split 100:1 @ 250 C, 1.0 L
Carrier Gas: Helium @ 1 mL/min (constant flow)Oven Program: 50 C to 250 C @ 6 C/min for 3 min
Detector: MSD @ 275 CSample: 1. Acetone
2. Ethyl acetate 3. Ethanol 4. Decane 5. Ethyl butyrate 6. Limonene 7. 2,3-Dimethylpyrazine 8. (Z)-3-Hexenol 9. Tetradecane10. Acetic acid11. Decanal12. Propylene glycol13. Ethyl decanoate14. Neral15. a-Terpineol16. Neryl Acetate17. Geranial18. Decanol19. Valeric acid20. Nonanoic acid21. Decanoic acid22. Vanillin23. Anthracene
Good Separation
Phenomenex l Web: www.phenomenex.com Phenomenex l Web: www.phenomenex.com18 19
18 20 22 24 min
1
2
3
4 5
6
7
8
9 10
11
12 13
14
16331
Vitamin E and Sterols by GC/FID Column: Zebron ZB-5
Dimensions: 30 meter x 0.25 mm x 0.10 mPart No.: 7HG-G002-02Injection: Splitless @ 220 C, 1 L
Carrier Gas: Helium @ 1.8 mL/min (constant flow)Oven Program: 110 C for 0.2 min to 140 C @ 30 C/min to 230 C @
10 C/min for 6 min to 340 C @ 10 C/min for 15.8 minDetector: FID @ 340 C
Sample: Analytes derivatized via BSTFA:TMCS; 99:1 in pyridine1. Squalene2. Lignoceric acid3. d-Tocopherol4. d-Tocomonoenol5. Campesta-3,5-diene6. g-Tocopherol7. Stigmasta-3,5,22-triene
8. g-Tocomonoenol 9. Stigmasta-3,5-diene10. Cholesterol11. a-Tocopherol12. Campesterol13. Stigmasterol14. b-Sitosterol
Margarine Sterols by GC/FID Column: Zebron ZB-5HT Inferno
Dimensions: 30 meter x 0.25 mm x 0.10 mPart No.: 7HG-G015-02Injection: Splitless @ 350 C, 0.5 L
Carrier Gas: Helium @ 2 mL/min (constant flow)Oven Program: 220 C to 350 C @ 15 C/min
Detector: FID @ 350 CSample: Prepared by saponification, solid phase extraction (SPE),
and derivatization via BSTFA: TMCS; 99:1 in pyridine 1. Campesterol 2. Stigmasterol 3. b-Sitosterol 4. Betulin
5.0 5.5
16750
2
3
4
1
6.0 6.5 7.0 7.5 min 6.05.5
1
3
4
2
16753
7.06.5 7.5 min
6.0 7.0 7.5 min5.5
16752
1
2
6.5
App
ID 1
6331
App
ID 1
6750
Lard Sterols by GC/FID Column: Zebron ZB-5HT Inferno
Dimensions: 30 meter x 0.25 mm x 0.10 mPart No.: 7HG-G015-02Injection: Splitless @ 350 C, 0.5 L
Carrier Gas: Helium @ 2 mL/min (constant flow)Oven Program: 220 C to 350 C @ 15 C/min
Detector: FID @ 350 CSample: Prepared by saponification, solid phase extraction (SPE), and
derivatization via BSTFA:TMCS; 99:1 in pyridine 1. Cholesterol 2. Betulin
Olive Oil Sterols by GC/FID Column: Zebron ZB-5HT Inferno
Dimensions: 30 meter x 0.25 mm x 0.10 mPart No.: 7HG-G015-02Injection: Splitless @ 350 C, 0.5 L
Carrier Gas: Helium @ 2 mL/min (constant flow)Oven Program: 220 C to 350 C @ 15 C/min
Detector: FID @ 350 CSample: Prepared by saponification, solid phase extraction (SPE),
and derivatization via BSTFA:TMCS; 99:1 in pyridine 1. Campesterol 2. Stigmasterol 3. b-Sitosterol 4. Betulin
App
ID 1
6752
App
ID 1
6753
SterolsSterols are naturally occurring steroid alcohols in plants, animals, and fungi. Phytosterols and cholesterol are commonly tested; sterol content for example is analyzed to determine olive oil quality and authenticity. Dietary tocopherols are sometimes tested with sterols due to their related health effects. Methods for analysis of sterols from common food matrices and in combination with tocopherols are demonstrated below.
Fats & Oils
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Butter Triglycerides by GC/FID Column: Zebron ZB-5HT Inferno
Dimensions: 15 meter x 0.32 mm x 0.10 mPart No.: 7EM-G015-02Injection: On-Column @ 103 C, 2 L
Carrier Gas: Helium @ 1.8 mL/min (constant flow)Oven Program: 100 C to 400 C @ 14 C/min for 10 min
Detector: FID @ 400 CSample: Butter
Peanut Oil Triglycerides by GC/FID Column: Zebron ZB-5HT Inferno
Dimensions: 30 meter x 0.25 mm x 0.10 mPart No.: 7HG-G015-02Injection: On-Column @ 63 C, 0.1 L
Carrier Gas: Helium @ 1.5 mL/min (constant flow)Oven Program: 60 C to 400 C @ 25 C/min for 10 min
Detector: FID @ 400 CSample: Peanut Oil
105 15
16054
20 25 30 min 0 5
16056
10 15 2520 min
0 5
16120
10 15 20 min 0 5
16121
10 15 20 min
App
ID 1
6054
App
ID 1
6120
Olive Oil Triglycerides by GC/FID Column: Zebron ZB-5HT Inferno
Dimensions: 30 meter x 0.25 mm x 0.10 mPart No.: 7HG-G015-02Injection: On-Column @ 223 C, 0.1 L
Carrier Gas: Helium @ 1 mL/min (constant flow)Oven Program: 220 C for 1 min to 400 C @ 8 C/min for 4 min
Detector: FID @ 415 CSample: Olive Oil
Olive Oil Sterols by GC/FID Column: Zebron ZB-5HT Inferno
Dimensions: 30 meter x 0.25 mm x 0.10 mPart No.: 7HG-G015-02Injection: Splitless @ 350 C, 0.5 L
Carrier Gas: Helium @ 2 mL/min (constant flow)Oven Program: 220 C to 350 C @ 15 C/min
Detector: FID @ 350 CSample: Prepared by saponification, solid phase extraction (SPE),
and derivatization via BSTFA:TMCS; 99:1 in pyridine 1. Campesterol 2. Stigmasterol 3. b-Sitosterol 4. Betulin
Canola Oil Triglycerides by GC/FID Column: Zebron ZB-5HT Inferno
Dimensions: 30 meter x 0.25 mm x 0.10 mPart No.: 7HG-G015-02Injection: On-Column @ 63 C, 0.1 L
Carrier Gas: Helium @ 1.5 mL/min (constant flow)Oven Program: 60 C to 400 C @ 25 C/min for 10 min
Detector: FID @ 400 CSample: Canola Oil
App
ID 1
6056
App
ID 1
6121
TriglyceridesTriglycerides are naturally-occurring esters of fatty acids and glycerol. Because these compounds have relatively high molecular weights and polarities that increase with the degree of unsaturation, high oven temperatures are necessary for sufficient separations. Choosing a GC column designed to withstand such temperatures (such as those with improved polyimide coatings that resist brittleness at 400 C or higher) can provide the necessary robustness to achieve good separation. The separations below are performed using a ZB-5HT Inferno GC column, which is specifically designed to stand up to high oven temperatures, are also shown.
Fats & Oils
Run at400
Run at400
Run at400
Run at415
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IntroductionDuring wine and distilled spirit fermentation, compounds called congeners are formed. These congeners can contribute to a spirits flavor, but can be harmful if consumed in excess. Some spirits, such as vodka, undergo extra processing steps to eliminate these compounds. Beyond health concerns, an overabundance of a specific congener can signify a problem with production or improper storage conditions. Distilleries also commonly perform congener profile analyses to mitigate adulteration claims and test for authenticity.
Because the congener profile of a distilled spirit is significant for both quality control and health safety, accurate analysis of these compounds is very important. Testing methods used to analyze these compounds must therefore be both qualitative, quantitative, and reproducible. GC/FID analysis of common congeners (such as those in Table 1) is known for its reproducibility and accuracy and is heralded as the industry standard. Polyethylene glycol (PEG) columns have historically provided acceptable selectivity but been unstable with aqueous samples, resulting in poor reproducibility and decreased lifetime. Traditional analysis is challenging because finished products are composed of 40 and 80 percent water, and congeners are present only in low parts per million (ppm).
Headspace sampling can eliminate some matrix effects and enhance the performance of the more volatile congeners, but will suppress the response of less volatile analytes which may be responsible for unique flavors. Direct injection is therefore still required to verify specific samples. This work explores the separation of distillation congeners on a Zebron ZB-WAXPLUSTM, a water-stable PEG phase.
Methods and MaterialsAnalyses were performed using an Agilent 6890 (Agilent Technologies, Palo Alto, CA, USA). Liquid injections used an Agilent liquid autosampler. Headspace samples used an HT-200 Automatic Headspace Sampler (Overbrook Scientific, Boston, MA, USA). All standards are > 95 % purity, and wine and distilled samples were purchased from local grocery stores. Instrument conditions for each method are included with the chromatogram.
Results and DiscussionSome of the primary congeners are very volatile and may be easily determined using headspace injection. A headspace injection of main congeners and flavor compounds is presented in Figure 1. This helps to keep most of the water and contaminants out of the system, which can contribute to decreased chromatographic performance and result in premature column deterioration. The earlier eluting peaks give excellent responses and can easily be quantified. Baseline resolution was achieved for acetaldehyde, ethyl acetate, and methanol (important components in monitoring the distillation process).
In some analyses, it is important to focus on the later eluting compounds because these have a large impact on the complicated flavors of fermented beverages. These congeners form as a result of the conditions of storage and aging and must be monitored to ensure product consistency. These later eluting compounds have lower volatility, and are better analyzed via liquid injections. A liquid injection of the same flavor standard is injected in Figure 2. Notice that the later eluting compounds have higher responses given the same concentration. This allows for a more accurate analysis of the flavor compounds which may be unique to a particular brand. For this reason, liquid injections are the preferred method for determining flavors.
On other PEG-based WAX columns, water can affect system performance and reproducibility. Zebron ZB-WAXPLUS columns are specially bonded to stand up to repeated aqueous injections. This can be seen in Figure 3, where multiple injections were made of a Scotch whiskey consisting of ~60 % water. There is no change in peak shape or retention times over time, and repeated injections have < 5 % RSD.
In addition to providing aqueous stability, ZB-WAXPLUS also provides very low activity for acidic compounds. This allowed for the fatty acids (eluting past 12 min) to be analyzed within the same run. The lack of acetic acid in the sample suggests that the product was well stored prior to opening and that the cork seal from the bottle was not compromised.
Additional beverages that have not been distilled can also be analyzed using the ZB-WAXPLUS. A chromatogram for an Italian wine is shown in Figure 4. In this instance, sample preparation consisted of only filtering before injecting. This chromatogram shows baseline separation of early eluting congeners, which can be used to monitor the fermentation process.
ConclusionMethod reproducibility and accuracy for distilled spirit analysis is very important for both quality control and health safety. Therefore, using an aqueous stable GC column is the best approach for congener analysis as it allows direct injection. Fermented beverages including distilled spirit congeners have historically been difficult to analyze by direct injection, but can be analyzed successfully using the Zebron ZB-WAXPLUS GC column. By using a Zebron ZB-WAXPLUS GC column for distilled spirit analysis, accuracy and reproducibility can be achieved without sacrificing resolution.
Analysis of Alcoholic Beverages (Distilled Spirits and Wines) Using a 100 % Aqueous Stable GC Column
Application Spotlight
Table 1: Common Distilled Spirit Congeners
Acetaldehyde Ethyl acetate Methanol Isobutanol
OHH
H HHC O
HOH
HH H
HC O
HOH
HH H
HC O
HOH
HH H
HC O
H
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Figure 1: Distilled Alcohol Standard by Headspace GC/FID Column: Zebron ZB-WAXPLUS
Dimensions: 30 meter x 0.25 mm x 0.25 mPart No.: 7HM-G013-11Injection: Split 25:1 @ 210 C, 1 L
Carrier Gas: Hydrogen @ 1 mL/min (constant flow)Oven Program: 35 C for 7 min to 60 C @ 5 C/min for 2 min to 210 C @ 10 C/min
Detector: FID @ 230 CNote: Static headspace injection (80 C for 20 min)
Sample:
Figure 2: Distilled Alcohol Standard by Liquid Injection Column: Zebron ZB-WAXPLUS
Dimensions: 30 meter x 0.25 mm x 0.25 mPart No.: 7HG-G013-11Injection: Split 25:1 @ 210 C, 1 L
Carrier Gas: Hydrogen @ 1 mL/min (constant flow)Oven Program: 35 C for 6 min to 60 C @ 5 C/min for 2 min to 210 C @ 10 C/min
Detector: FID @ 230 CNote: 200 ppm standard in methylene chloride
Sample:
10
1
2
3
5
6
7
8
9
10
11
12
1314
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
4
16324
20 min 10 155
1
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
20 21
22
24
25
26
27
28
2930
31
32
33
34
23
19
32
16325
20 25 min
Ap
p ID
163
24
Ap
p ID
163
25
1. Acetaldehyde 12. 1-Propanol 24. cis-3-Hexenol 2. Isobutanal 13. Isobutanol 25. Ethyl caprylate 3. Ethyl formate 14. Allyl alcohol 26. Furfural 4. Acrolein 15. Isoamyl acetate 27. Benzaldehyde 5. Ethyl acetate 16. Butanol 26. Furfural 6. Acetal 17. 4-Methyl-2-pentanol 27. Benzaldehyde 7. Methanol 18. Methyl-2-butanol 28. Ethyl caprate 8. Ethanol 19. Methyl-3-butanol 29. Diethyl succinate 9. Isobutyl acetate 21. Ethyl heptanoate 30. Ethyl laurate10. 2-Butanol 22. Ethyl lactate 31. Phenyl-2-ethanol11. Ethyl butyrate 23. Hexanol
1. Acetaldehyde 2. Ethyl acetate 3. Methanol 4. Ethanol
1. Acetaldehyde 2. Ethyl acetate 3. Methanol 4. Ethanol
5. Propanol 6. Isobutanol 7. 2-Methylbutanol 8. 3-Methylbutanol
5. Propanol 6. Isobutanol7. 3-Methyl-1-butanol
1. Acetaldehyde 13. 1-Propanol 25. cis-3-Hexenol 2. Isobutanal 14. Isobutanol 26. Ethyl caprylate 3. Ethyl formate 15. Allyl alcohol 27. Furfural 4. Acrolein 16. Isoamyl acetate 28. Benzaldehyde 5. Ethyl acetate 17. 1-Butanol 29. Linalool 6. Acetal 18. 4-Methyl-2-pentanol 30. Linalyl acetate 7. Methanol 19. Methyl-2-butanol 31. Ethyl caprate 8. Methylene chloride 20. Methyl-3-butanol 32. Diethyl succinate 9. Ethanol 21. Ethyl caproate 33. Ethyl laurate10. Isobutyl acetate 22. Ethyl heptanoate 34. 2-Phenyl ethanol11. 2-Butanol 23. Ethyl lactate12. Ethyl butyrate 24. Hexanol
Figure 4: Filtered Liquid Injection of Italian Wine Column: Zebron ZB-WAXPLUS
Dimensions: 30 meter x 0.32 mm x 0.25 mPart No.: 7HM-G013-11Injection: Split 10:1 @ 150 C, 0.2 L
Carrier Gas: Helium @ 2.3 mL/min (constant flow)Oven Program: 40 C for 5 min to 150 C @ 5 C/min for 5 min to 220 C @
20 C/min for 2 minDetector: FID @ 280 C
Accessories: Phenex-RC Syringe Filter (AF0-2203-52)Note: Wine has been filtered through 0.2 m regenerated cellulose filter
and directly injected.Sample:
Figure 3: Replicate Liquid Injections of Undiluted Scotch Whiskey Column: Zebron ZB-WAXPLUS
Dimensions: 30 meter x 0.25 mm x 0.25 mPart No.: 7HG-G013-11Injection: Split 30:1 @ 140 C, 0.2 L
Carrier Gas: Helium @ 1.4 mL/min (constant flow)Oven Program: 35 C for 5 min to 85 C @ 10 C/min to 200 C @ 25 C/min for 1 min
Detector: FID @ 200 CSample:
3
3
2
1
18299
4
4
5
5
6
6
7
7
8 9 10 11 min
Ap
p ID
182
99
m in0 2
1 2 3
4
5
6
7,8
4 6 8 10 12 14
pA
0
10
20
30
40
50
60
70
80
90
Ap
p ID
158
17
Scottish Single Malt Whiskey 60 % Aqueous!
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Many additives and preservatives are commonly tested using GC. Borneol, a naturally occurring terpene derived from plant essential oils, is used as a flavor or fragrance additive in small amounts. Though not approved by the U.S. Food and Drug Administration, borneol is not prohibited as an ingredient in herbal/dietary supplements, and additionally used in traditional Chinese medicines for its antibiotic, sedative, and pain-relieving properties. However, risk of allergenic side effects to the respiratory and skin systems has increased its testing.
Additives & Preservatives
Borneol by GC/MS Column: Zebron ZB-MultiResidue-1
Dimensions: 30 meter x 0.25 mm x 0.25 mPart No.: 7HG-G016-11Injection: Splitless @ 270 C (hold 0.66 sec), 1.0 L
Carrier Gas: Helium @ 0.3 mL/min (constant flow)Oven Program: 60 C for 2 min to 270 C @ 10 C/min
Detector: MSD @ 230 C, 45-450 amuSample: 1. Isoborneol
2. Borneol
6
16360
1
2
8 10 12 14 16 18 20 22 min
App
ID 1
6360
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Food SafetyFeatured Applications
Interested in Food Safety?
www.phenomenex.com/Food
Request the Food Safety Solutions Guide for comprehensive GC, LC, and sample Preparation applications
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PhthalatesPhthalates are internationally regulated carcinogenic, teratogenic, and mutagenic plasticizers that can migrate from packaging into food and beverage products. GC/MS has been widely used for phthalate residue testing, but late elution of the heavier compounds can lead to low detection limits. Many of the compounds additionally require chromatographic separation due to virtually identical fragmentation patterns. The below method features a fast, 11 minute run with good thermal stability.
Melamine and Cyanuric AcidThough low in toxicity individually, melamine and cyanuric acid crystallize in a 1:1 ratio in concentrations exceeding 2 g/mL to form melamine cyanurate, a very poorly water-soluble complex. Consumption of melamine cyanurate can result in adverse health problems, including kidney failure and death. The GC/MS method below yields fully resolved peaks in less than 9 minutes and allows for the high-temperature removal of residual on-column contaminants for longer column lifetime.
Food Contact Materials
Phthalates by GC/MSColumn: Zebron ZB-50
Dimensions: 30 meter x 0.25 mm x 0.25 mPart No.: 7HG-G004-11Injection: Split 10:1@ 260 C, 1 L
Carrier Gas: Helium @ 1 mL/min (constant flow)Oven Program: 135 C to 275 C @ 25 C/min for
3.5 min to 340 C @ 35 C/min for 1 minDetector: MSD @ 320 C , 45-500 amu
1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.51.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 min
19931
2
3
45
6,78
9
10 11
12
14
1516
17 18
19
13
1
20 21 App
ID 1
9931
Sample 1. Dimethyl phthalate 2. Diethyl phthalate 3. Diallyl phthalate 4. Di-n-propyl phthalate 5. Di-n-butyl phthalate 6. Diisobutyl phthalate 7. Di-n-hexyl phthalate 8. Bis(2-methoxyethyl) phthalate9. Di-n-pentyl phthalate
10. Bis(2-ethoxyethyl) phthalate 11. Di-(4-methyl-2-pentyl) phthalate 12. Bis(2-ethylhexyl) phthalate 13. Benzyl butyl phthalate 14. Di-n-heptyl phthalate15. Bis(2-n-butoxyethyl) phthalate 16. Dicyclohexyl phthalate 17. Di-n-octyl phthalate 18. Diphenylhexyl phthalate19. Di-n-nonyl phthalate 20. Diisononyl phthalate21. Diisodecyl phthalate
Column: Zebron ZB-XLB-HT Inferno
Dimensions: 15 meter x 0.25 mm x 0.25 mPart No.: 7EG-G024-11Injection: On-Column @ 103 C, 1 L
Carrier Gas: Helium @ 1.4 mL/min (constant flow) Oven Program: 100 C for 0.5 min to 320 C @ 25 C/min
Detector: MSD @ 325 CSample: Analytes are 200 ng / 100 L in BSTFA / Pyridine (1:1)
1. Cyanuric Acid 13C3 (IS) 2. Cyanuric Acid 3. Melamine 13C3 15N3 (IS) 4. Melamine
3 42
1,2
3,4
18265
5 6 7 8 9min
App
ID 1
8265
Bis(2-ethylhexyl) phthalate
Diisobutyl phthalate
Dicyclohexyl phthalate
Dimethyl phthalate
Di-n-octyl phthalate
Benzyl butyl phthalate
Explore PremiereZebron GC Columns
Complete analysis in less than half the time
of the FDA method
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App
ID 1
6184
8 10 12 14 16 18 20 22 24 26 28 30 32 34
14 16 18 min
min
22 24 min
18
19
20
21
22
23
24 25
27
28
29 3031
32
34
35
40
33
48
51
49
50
52
38
39
26
36,37 41-43
44-45
46-47
58
59
60
61
62
63
64-66
67
68
69
70
75
76
77,78
79
82
84
83
85
86 87
71-74
80-81
12
3
4
5
6,7
5354
55
57
56
9
10
12
13-15
17
1188
94,95
96
97
98
99100
101
102103
104
105
106
107
108
109
110,111
11292,93
90
91
89
8
16
1. Dichlorvos 2. DEET 3. EPTC 4. 3,5-Dichlorobenzoic acid (methyl ester) 5. Butylate 6. 4-Nitrophenol (methyl ester) 7. Vernolate 8. Mevinphos 9. Mevinphos isomer 10. Pebulate 11. Trichlorfon 12. Dicamba (methyl ester) 13. Molinate 14. Tebuthiuron 15. MCPP (methyl ester) 16. Tetraethyl pyrophosphate (methyl ester) 17. MCPA (methyl ester) 18. Demeton Isomer 19. Thionazin (zinophos) 20. Dichloroprop (methyl ester) 21. Propachlor
22. Cycloate 23. Ethoprop 24. Trifluralin 25. Benefin 26. 2,4-D (methyl ester) 27. Sulfotep 28. Naled 29. Chlorpropham 30. Dicrotophos 31. Phorate 32. Monocrotophos 33. Pentachlorophenol (methyl ester) 34. Demeton 35. Atraton 36. Profluralin 37. Prometon 38. Silvex (methyl ester) 39. Terbufos 40. Dimethoate 41. Simazine 42. Propazine 43. Atrazine
44. Diazinon 45. Dioxathion 46. Terbuthylazine 47. Fonofos 48. Pronamide (propyzamide) 49. Chloramben (methyl ester) 50. 2,4,5-T Methyl ester 51. Phosphamidon isomer 52. Disulfoton 53. Secbumeton 54. Terbacil 55. Dinoseb (methyl ester) 56. Dichlofenthion 57. 2,4-DB (methyl ester) 58. Phosphamidon 59. Chlorpyrifos methyl 60. Alachlor 61. Bentazon (methyl ester) 62. Ronnel 63. Prometryn 64. Methyl parathion 65. Ametryn 66. Simetryn
67. Aspon 68. Metribuzin 69. Terbutryn 70. Malathion 71. Fenitrothion 72. Picloram (methyl ester) 73. Metolachlor 74. Chlorpyrifos 75. DCPA 76. Bromacil 77. Fenthion 78. Trichloronate 79. Triadimeton 80. Isopropalin 81. Parathion 82. MGK-624 83. Merphos 84. Pendimethalin (Penoxaline) 85. Diphenamide 86. MGK-264 isomer 87. Clofenvinfos 88. Crotoxyphos 89. Butachlor
Sample:
Multi-Residue ScreeningThough globally regulated due to their detrimental health effects, restrictions on pesticide use differ from one country to the next. Since many different types of pesticides can be used on the same food product, multi-residue screening approaches by GC/MS are used to analyze large lists of 100 compounds or more in a single run. As demonstrated below, optimized selectivity offers increased resolution of critical compounds vs. standard 5ms phases.
Pesticides & Antimicrobials
Multi-Residue Pesticide Screen by GC/MS Column: Zebron ZB-MultiResidue-1
Dimensions: 30 meter x 0.25 mm x 0.25 mPart No.: 7HG-G016-11Injection: Splitless @ 260 C, 1 L
Carrier Gas: Helium @ 0.9 mL/min (constant flow) Oven Program: 80 C for 0.5 min to 150 C @ 10 C/min to
240 C @ 4 C/min to 320 C @ 15 C/min for 3 minDetector: MSD @ 320 C; 45-400 amu
Note: Analytes were 1 ppm in dichloromethane
90. Stirofos 91. Tokuthion 92. Napropamide 93. Fenamiphos 94. Merphos oxide 95. Oxadiazon 96. Oxyfluorfen 97. Carboxin 98. Tricyclazole 99. Acifluorfen 100. Ethion 101. Fensulfothion 102. Carbofenothion 103. Famfur 104. Norflurazon 105. Hexazinone 106. EPN 107. Phosmet 108. Leptophos 109. Azinphos-methyl 110. Fenarimol 111. Azinphos-ethyl 112. Coumaphos
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Polycyclic Aromatic Hydrocarbons (PAHs)PAHs are a class of persistent organic pollutants (POPs) that are implicated as carcinogens. Due to their potential health risk at low levels, PAH testing is often performed from a variety of food matrices. PAH isomers are additionally well-known for their challenging isomers and interferences. Separations of common troublesome analytes are demonstrated below.
Environmental Contaminants
Column: Zebron ZB-SemiVolatilesDimensions: 30 meter x 0.25 mm x 0.25 m
Part No.: 7HG-G027-11 Injection: Split 10:1 L @ 280 C, 1 L
Carrier Gas: Helium @ 1.4 mL/min (constant flow)Oven Program: 100 C for 0.5 min to 260 C @ 30 C/min to 295 C @ 6 C/min to
325 C @ 25 C/min for 2 minDetector: MSD @ 340 C; 45-450 amu
Note: Analytes are 25 ppm in Dichloromethane
Sample: 11. Benz[a]anthracene 12. Chrysene 13. Benzo[b]fluoranthene 14. Benzo[k]fluoranthene 15. Benzo[a]pyrene 16. 3-Methylcholanthrene 17. Indeno[1,2,3-cd]pyrene 18. Dibenz[a,h]anthracene 19. Benzo[g,h,i]perylene
3
20578
1
2
3
4
56
7
8
910
11
12
13
14
15
16
1718 19
4 5 6 7 8 9 10 11 12 13 14 min
App
ID 2
0578
Column: Zebron ZB-35Dimensions: 30 meter x 0.25 mm x 0.25 m
Part No.: 7HG-G003-11Injection: On-Column @ 83 C, 1 L
Carrier Gas: Helium @ 1.2 mL/min (constant flow)Oven Program: 80 C for 0.66 min to 250 C @ 20 C/min to
360 C @ 8 C/min for 6 minDetector: MSD @ 360 C; 45-450 amu
Note: Analytes are 10 ppm in Dichloromethane
Sample: 1. Naphthalene 2. 2-Methylnaphthalene 3. Acenaphthylene 4. Acenaphthene 5. Fluorene 6. Phenanthrene 7. Anthracene 8. Fluoranthene 9. Pyrene 10. Benz[a]anthracene 11. Chrysene 12. Benzo[b]fluoranthene 13. Benzo[k]fluoranthene
14. Benzo[j]fluoranthene 15. Benzo[a]pyrene 16. 3-Methylcholanthrene 17. Dibenz[a,h]acridine 18. Dibenz[a,j]acridine 19. Indeno[1,2,3-cd]pyrene 20. Dibenz[a,h]anthracene 21. Benzo[g,h,i]perylene 22. 7H-Dibenzo[c,g]carbazole 23. Dibenzo[a,e]pyrene 24. Dibenzo[a,i]pyrene 25. Dibenzo[a,h]pyrene
App
ID 1
8525
6 8 10 12 14 16 18 20 min
18525
1112 1314
15
16
1718
19,20
21
2223
24
25
1098
6
7
543
21
PAHs by GC/MS
PAHs by GC/MS
Benz[a]anthracene and chrysene are totally resolved
Resolve benzo[b], benzo[j], and benzo[k]fluoranthene
1. Naphthalene 2. 2-Methylnaphthalene 3. 1-Methylnaphthalene 4. Acenaphthylene 5. Acenaphthene 6. Fluorene 7. Phenanthrene 8. Anthracene 9. Fluoranthene 10. Pyrene
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0.0E+00
5.0E+04
1.0E+05
1.5E+05
2.0E+05
27 27.2 27.4 27.6 27.8 28 28.2 28.4 28.6 28.8 29
BDE-209S/N = 20
0.0E+00
2.0E+06
4.0E+06
6.0E+06
8.0E+06
1.0E+07
1.2E+07
25 25.2 25.4 25.6 25.8 26 26.2 26.4 26.6 26.8 27
BDE-209S/N = 815
Ap
p ID
219
25
0.0E+00
5.0E+07
1.0E+08
1.5E+08
2.0E+08
2.5E+08
3.0E+08
3.5E+08
4.0E+08
10 12 14 16 18 20 22 24 26 28 min
Inte
nsity
BDE-209
Zebron ZB-SemiVolatiles
Ap
p ID
219
26
0.0E+00
1.0E+08
2.0E+08
3.0E+08
4.0E+08
5.0E+08
6.0E+08
7.0E+08
8.0E+08
9.0E+08
1.0E+09
10 12 14 16 18 20 22 24 26 28 min
Inte
nsity
BDE-209
Agilent DB-5ms Ultra Inert
Polybrominated Diphenyl Ethers (PBDEs)PBDEs consist of 209 individual congeners which vary in toxicity. Though congener testing is performed by high resolution GC (HRGC/HRMS), achieving accurate, well-resolved separations is historically problematic due to the sheer number of compounds and analyte stability. The fast method below includes the quantitation of BDE-209 in a single analytical run, with improved column stability compared to traditionally used phases.
Environmental Contaminants
Column: A: Zebron ZB-SemiVolatilesB: Agilent DB-5ms Ultra Inert
Dimensions: 20 meter x 0.18 mm x 0.18 mInjection: Splitless @ 85 C, 5 L
Carrier Gas: Helium @ 0.85 mL/min (constant flow) Oven Program: 70 C for 1.25 min to 240 C @ 20 C/min to
320 C @ 50 C/min for 18 minDetector: High Res Mass Spec (HRMS) @ 325 C
Note: Used a PTV in Solvent Vent Mode with temperatureprogram to 320 C in 2 min
PBDEs by GC/HRMS
Comparative separations may not be representative of all applications.
> 40x GreaterSignal-to-Noise
Conditions for both columns:
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Environmental Contaminants
0.0E+00
5.0E+07
1.0E+08
1.5E+08
2.0E+08
2.5E+08
3.0E+08
10.4 10.45 10.5 10.55 10.6 10.65 10.7 10.75 min
0.0E+00
2.0E+07
4.0E+07
6.0E+07
8.0E+07
1.0E+08
1.2E+08
1.4E+08
1.6E+08
1.8E+08
2.0E+08
10.8 10.9 11 11.1 11.2 11.3 11.4 11.5 min
0.0E+00
5.0E+07
1.0E+08
1.5E+08
2.0E+08
2.5E+08
3.0E+08
3.5E+08
4.0E+08
11.6 11.7 11.8 11.9 12 12.1 12.2 min
0.0E+00
5.0E+07
1.0E+08
1.5E+08
2.0E+08
2.5E+08
12.3 12.5 12.7 12.9 13.1 13.3 min
0.0E+00
2.0E+07
4.0E+07
6.0E+07
8.0E+07
1.0E+08
1.2E+08
13.5 13.7 13.9 14.1 14.3 14.5 14.7 min
0.0E+00
1.0E+07
2.0E+07
3.0E+07
4.0E+07
5.0E+07
6.0E+07
23 23.5 24 24.5 25 25.5 26 26.5 27 27.5 min
Tribromophenyl ethers Hexabromophenyl ethers
13C-BDE-28+ BDE-28
13C-BDE-154+ BDE-154 13C-BDE-153
+ BDE-153
BDE-138
Tetrabromophenyl ethers Heptabromophenyl ethers
13C-BDE-47+ BDE-47
13C-BDE-77
+ BDE-77
13C-BDE-183+ BDE-183
BDE-190
BDE-75 BDE-71 BDE-66
Pentabromophenyl ethers Decabromophenyl ether
13C-BDE-100 + BDE-100 13C-BDE-99
+ BDE-99
13C-BDE-209+ BDE-209
BDE-119BDE-85
App
ID 2
1925
Panu RantakokkoNational Institute for Health and Welfare, Finland
We have had great difficulties with the stability of BDE-209 with our previous GC columns, and we were forced to use a very short column (6 m) for this specific compound instead of a regular 20-30 m column. To be able to run all PBDEs in one run we decided to test ZebronTM ZB-SemiVolatiles.
With a narrow bore 20 m x 0.18 mm ID x 0.18 m film ZB-SemiVolatiles column we are now able to successfully analyze our suite of PBDEs from BDE-28 to BDE-209 in a single run. Peak height of BDE-209 with this column is 10-30 times higher than with a brand new column of similar (5 % phenyl) chemistry and dimensions from another well-known manufacturer. Use of ZB-SemiVolatiles roughly halves the time required for analysis as there is no longer a need for a second injection with a shorter column.
ZB-SemiVolatiles represents a major improvement in the GC analysis of highly brominated flame retardants.
PBDEs by GC/HRMS
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Polychlorinated Biphenyls (PCBs)PCBs are commonly tested in addition to chlorinated pesticides, and are analyzed either as individual congeners, or as Aroclor mixtures. A number of methods for PCB analysis exist, including EN 1528, AOAC 970.52, ISO 10382, and EPA 1668 and 8082, among others. Some congeners have toxicity characteristics similar to 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD). These dioxin-like PCBs have been assigned Toxic Equivalency Factors (TEF) relative to the 2,3,7,8-TCDD isomer. Aroclor mixtures are first qualitatively identified by their unique fingerprint in comparison to a standard. Any contaminants present in the run may interfere with Aroclor fingerprints, making data analysis difficult.
Environmental Contaminants
Aroclor 1254
Aroclor 1260
Aroclor 1254
Aroclor 1260
App
ID 2
2645
App
ID 2
2652
PCBs by Dual-Column GC/ECD
APP
ID 2
2642
APP
ID 2
2649
min
22645
2
1 2
4 6 8 10 min
1 2
22652
2 4 6 8 10
Conditions for all columns:Columns: As listed
Dimensions: 30 meter x 0.25 mm x 0.25 m (ZB-CLPesticides-1)30 meter x 0.32 mm x 0.32 m (ZB-CLPesticides-2)
Part Number: 7HM-G028-51 (ZB-CLPesticides-1)7HM-G029-11 (ZB-CLPesticides-2)
Injection: Pulsed Splitless @ 30 psi (hold 20 sec) @ 250 C, 1 L Carrier Gas: Helium @ 60 cm/sec (constant flow)
Oven Program: 120 C to 200 C @ 45 C/min to 330 C @15 C/min for 2 min
Detector: ECD @ 330 CY-Connector: AG0-4717 (Borosilicate Glass)
Guard Column: 7AM-G000-00-GZ0 (5 m Z-Guard)Liner: AG0-8499 (Single Taper with Wool at Bottom)
Septum: AG0-4696 (PhenoRed-400)Inlet Seal: AG0-8620 (Gold-Plated Easy Seals)
Sample: Aroclor is 1000 ng/mL and SS and IS are 100 ng/mL in hexane.1. Tetrachloro-meta-xylene (TCMX) (surrogate standard)2. Decachlorobiphenyl (internal standard)
CLP-1
CLP-1
CLP-2
CLP-2
min
22642
2
1 2
4 6 8 10 min
22649
2
1 2
4 6 8 10
Phenomenex l Web: www.phenomenex.com Phenomenex l Web: www.phenomenex.com30 31
11999907074
37
7 min
31
15
1 35
14777
53
14 min12 16108
181110 149
123168
114 141 158167
177157 201 189 207
194
App
ID 1
4777
11999907074
37
7 min
31
15
1 35
14777
53
14 min12 16108
181110 149
123168
114 141 158167
177157 201 189 207
194
App
ID 1
4777
184
min
209206
195170169199180
156128202
126187138105 183
864
153165
11815177
87115
10166
44495228188
TCMXa)
14775
min141210 16
App
ID 1
4775
184
min
209206
195170169199180
156128202
126187138105 183
864
153165
11815177
87115
10166
44495228188
TCMXa)
14775
min141210 16
App
ID 1
4775
PCB Congeners by GC/MS
PCB Congeners by GC/ECD
10 15 20 25 30 35 40 45 50 55 60 65 70 min
105(penta)
123(penta)
118(penta)
115 (penta), 87 (penta), 148 (hexa) 122 (penta), 165 (hexa), 188 (hepta)110 (penta), 154 (hexa)
77(tetra)
139 (hexa), 149 (hexa)
107 (penta)
127 (penta)
133 (hexa)
114 (penta)131 (hexa)
106 (penta), 140 (hexa)
47 48 49 50 51 52 53
81 (tetra)
min 56 57 58 59 60 61 62 63 64 65 66
175 (hepta)
166 (hexa) 128
(hexa)185
(hepta)126
(penta)
167(hexa)
156(hexa)
169(hexa)
189(hepta)
157(hexa)204 (octa)
171(hepta)
173 (hepta) 200 (octa)
180(hepta) 193 (hepta)
170(hepta) 190 (hepta)
192(hepta) 198
(octa)
191(hepta)
min
Column: Zebron ZB-5msDimensions: 60 meter x 0.25 mm x 0.25 m
Part No.: 7KG-G010-11Injection: Splitless @ 280 C for 0.5 min (1 L)
Carrier Gas: Helium @ 1.1 mL/min (constant flow)Oven Program: 60 C for 1 min to 140 C @ 25 C/min
to 290 C @ 2 C/minDetector: MSD @ 320 C; 35-510 amu
Sample: PCB Congeners
Conditions for both columns:Column: As listed
Dimensions: 30 meter x 0.32 mm x 0.25 mPart No.: 7HM-G004-11 (ZB-50)Injection: Splitless @ 225 C, 1.0 L
Carrier Gas: Helium @ 2.5 mL/min (constant flow)Oven Program: 130 C to 230 C @ 20 C/min to 270 C @
4 C/min to 300 C @ 20 C/min (hold 1min)Detector: ECD @ 325 C
Sample: PCB Congeners
Former WHO Toxic Congener Under 1994 ReportCurrent WHO Toxic Congener Under 1997 ReportNon-Dioxin-Like PCB Congener
App
ID 2
1432
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IntroductionDioxins (PCDDs) are a particularly toxic class of priority organic pollutants (POPs) that are extremely persistent in the environ-ment. They enter our food chain primarily through combustion of organic materials in waste incineration. Several other classes of POPs including dibenzofurans (PCDFs) and polychlorinated biphenyls (PCBs) display dioxin-like biological activity and are often monitored in conjunction with dioxins to give an overall toxic equivalent (TEQ) for a sample.
The European Union (EU) has published regulatory limits for the presence of these dioxin-like compounds in food and feed products. Recent contamination of 2,256 tons of fat incorporated in feed products in Germany has once again drawn attention to the need for routine monitoring. Dioxins are highly fat soluble and tend to bioaccumulate as they work their way up the food chain, posing a health risk to anyone consuming products from animals that were fed contaminated feed.
Robust analytical testing procedures are needed to determine potential threats in both feed and animal fat. In this article we discuss a rapid extraction and analysis procedure that allows all dioxin-like compounds to be determined in a single test. This methodology was used to analyze non-organic chicken feed as well as Mississippi River fish. The same methodology has also been applied to fish from the Great Lakes and shrimp collected internationally, though the data is not presented here.
Methods and MaterialsA 10 gram sample aliquot was spiked with labeled internal standards and extracted for 16 hours in toluene. The extracts were cleaned up and analyzed for PCDDs, PCDFs and PCBs using high resolution mass spectrometry (HRMS). PCDD and PCDF analysis was performed using a Zebron ZB-5ms 60 meter x 0.25 mm x 0.25 m (p/n: 7KG-G010-11) GC column in accordance with US EPA Method 1613B. PCB analysis was performed using a Zebron ZB-1 60 meter x 0.25 mm x 0.25 m (p/n: 7KG-G001-11) GC column in accordance with US EPA Method 1668A.
Results and DiscussionThe general dioxin structure has two benzene rings connected by two oxygen atoms and substituted at various positions with one to eight chlorine atoms (Figure 1). The position of the chlorine atoms around the two benzene rings determines the toxicity of the isomer with the tetra and penta chlorinated dioxin (TCDD/PeCDD) substituted at the 2, 3, 7, and 8 positions being the most toxic. Penta through Octa substituted isomers with chlorines at the 2,3,7,8 position are assigned toxicity equivalent factor (TEF) relative to the 2,3,7,8-TCDD isomer (Table 1). Similar TEF values have also been determined for other dioxin-like compounds. The relative toxicity or toxic equivalent (TEQ) of a sample can then be determined by summing the concentration of each congener multiplied by its TEF value (Equation 1).
Analysis of Dioxins, Dibenzofurans, and Polychlorinated Biphenyls from Animal Feed and Tissue Using High Resolution Gas Chromatography (HRGCMS)
Application Spotlight
Figure 1: General Structure for a Dioxin Isomer
8
7
2
3
9O
O
1
6CIx 4 CIy
Equation 1: TEQ = Ci x I-TEFi, where Ci is the concentration of a 2,3,7,8 substituted dioxin isomer
The analysis of these dioxin-like compounds was done using a gas chromatograph (GC) connected to an HRMS. This allowed for extremely high resolution between dioxin isomers, which allowed for accurate quantitation. However, even the advanced HRMS is unable to differentiate between isomers having the same degree of chlorination. This requires a high efficiency GC column capable of resolving compounds with the same chemi-cal properties, but slightly different geometry. The Zebron ZB-5ms column uses an arylene matrix bonding technology that significantly improves resolution between dioxin isomers (Figure 2).
Figure 2: Resolution Check Mix for TCDD Isomers Zebron ZB-5ms
26.12 26.24 26.36 26.48 27.00 27.12 27.24
1,2,3,9
1,2,3,7/1,2,3,81,2,3,4
2,3,7,8
27.36 27.48 min
Traditional 5ms
24.16 24.37 24.57 25.18 25.38 25.58 26.19
1,2,3,91,2,3,7/1,2,3,8
1,2,3,4
2,3,7,8
26.39 min
Using this optimized procedure, we compared the TEQ for fish samples from the Southern Mississippi river. There was very little, if any, difference between farm-raised and wild-caught fish (Table 2). This may be due to downstream effects, the possibility of point sources near to where the fish were
App
ID 1
5584
App
ID 1
5555
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collected, and even the age of the fish collected. For the Missis-sippi River, tissue levels were on average, lower than expected. This may be due to several factors including the larger volume of water in this river and the rapid currents compared to those of smaller and shallower rivers1.
We then applied this methodology to a non-organic chicken feed used by various farms near Vista Analytical Laboratory (Table 3). We only observed three of the World Health Orga-nization (WHO) dioxin-like compounds: 1,2,3,4,6,7,8-HpCDD, OCDD, and PCB 118. The calculated TEQ value for the sample was 0.00461, which was well below the EU maximum. These levels are a consistent continuation of the downward trend of PCDD/F and PCB levels in food products initially reported by several researchers in the mid-1990s.2,3,4
Table 1: Toxic Equivalency Factors for Dioxin-Like Compounds
Congener WHO-TEF Congener WHO-TEF
2005 20052,3,7,8-TCDD 1 PCB-77 0.00011,2,3,7,8-PeCDD 1 PCB-81 0.00031,2,3,4,7,8-HxCDD 0.1 PCB-105 0.000031,2,3,6,7,8-HxCDD 0.1 PCB-114 0.000031,2,3,7,8,9-HxCDD 0.1 PCB-118 0.000031,2,3,4,6,7,8-HpCDD 0.01 PCB-123 0.00003OCDD 0.0003 PCB-126 0.12,3,7,8-TCDF 0.1 PCB-156 0.000031,2,3,7,8-PeCDF 0.03 PCB-157 0.000032,3,4,7,8-PeCDF 0.3 PCB-167 0.000031,2,3,4,7,8-HxCDF 0.1 PCB-169 0.031,2,3,6,7,8-HxCDF 0.1 PCB-189 0.000032,3,4,6,7,8-HxCDF 0.11,2,3,7,8,9-HxCDF 0.11,2,3,4,6,7,8-HpCDF 0.011,2,3,4,7,8,9-HpCDF 0.01OCDF 0.0003
Table 2: TEQ Values for Fish Caught in the Mississippi River
Samples (N)
Mean TEQ (pg/g)
Range
Wild-Caught 33 1.50 0.13 - 4.96Farm-Raised 31 0.98 0.15 - 2.56
ConclusionThanks to aggressive regulatory action, the level of dioxin-like compounds in the environment is on the decline. Most high level samples are the result of remediation efforts or accidents, such as was observed in Germany. When such testing is required, testing laboratories must use the most advanced techniques available in order to quickly and accurately determine the potential risk to the general population.
Table 3: Dioxin-Like Compounds Found in Non-Organic Chicken Feed
Dioxin-Like Compound Concentration (pg/g)2,3,7,8-TCDD ND1,2,3,7,8-PeCDD ND1,2,3,4,7,8-HxCDD ND1,2,3,6,7,8-HxCDD ND1,2,3,7,8,9-HxCDD ND1,2,3,4,6,7,8-HpCDD 0.421OCDD 1.052,3,7,8-TCDF ND1,2,3,7,8-PeCDF ND2,3,4,7,8-PeCDF ND1,2,3,4,7,8-HxCDF ND1,2,3,6,7,8-HxCDF ND2,3,4,6,7,8-HxCDF ND1,2,3,7,8,9-HxCDF ND1,2,3,4,6,7,8-HpCDF ND1,2,3,4,7,8,9-HpCDF NDOCDF NDPCB-77 NDPCB-81 NDPCB-105 NDPCB-114 NDPCB-118 2.90PCB-123 NDPCB-126 NDPCB-156 NDPCB-157 NDPCB-167 NDPCB-169 NDPCB-189 ND
TEQ 0.00461
References1. Ferrib